Bitumen of high softening point



Dec. l5, 1942. H. M. NOEL l BITUMEN OF HIGH SOFTENING POINT Filed July 25,1940

meme Dec. 1s, 1942 UNITED STATES PATENT OFFICE 2,305,440 i BITUMEN F HIGH SOFTENING POINT Henry M. Noel, Summit, N. I., assignor to Stand'- ard 0ii Development Company, a corporation of Delaware Application July 25, 1940, smal' No. 341,353

ILClaims.

This invention relates to hard unoxidized bituminous materials, a process for preparing the same and more particularly it relates to an asphalt having a high softening point and a definite change in penetration with vtemperature.

It is especially suitable for the manufacture of molded asphalt products generally.' such as electric storage battery boxes, and also in the manufacture of high grade baking enamels and Japans.

Asphalts to be used for electric storage box compounds, molded products and in the manuv minedby test No. D5-25 of the American Society for Testing Materials (A. S. T. M.)

According to the same standard, the susceptibility factor should be between 27 and 35 as calculated by the following formula:

Penetration at 150 F./100 3./5 secs. L Penetration at 115' F./200 g./5 secs.

Penetration at 185 F./50 g./5 secs.

Penetration at 150 F./100 g./5 secs. K

The softening point should be above about 260 F. as determined by the ring and ball method, test No. D36-26 of the A. S. T. M.

The ductility should be high, that is about 35 to 40 centimeters at 185 F. at the rate` of 5 cm./min. as determined by test No. D113-35 of the A. S. T. M.

It is well known to crack a reduced crudevoil 'to produce lighter hydrocarbons and a heavy fuel oil which is further distilled to produce a pitch are all combined that the desired product is secured.

According to this invention paraffin-free vasphaltic base crudes, especially those from the western part of Venezuela. are suitable for the production of asphalt having the desired soften- .ing point and susceptibility, and other characteristics. The crude coming from the Lagunillas field is particularly' desirable. rUnless this" crude is treated under proper conditions however, the desired product will not be obtained. asphaltic content must be cracked to a certain point but cracking beyond this point results in an asphalt which is not suitable for this purpose. The final distillation also must be carried out `under conditions `which will give the desired nelting point without appreciable further crack-v Theoptimuxn conditions will vary somewhat with. varying feed stocks, which can best be determined by experiment whenever the quality of the starting material changes.

The present invention will be understood on reading the following description of a typical example and by referring to the drawing of a 'diagrammatical representation of one type of app'aratus suitable for the herein described process.

vA suitable oil, a parafiin-free asphaltic base crude, for example, Lagunillas crude, is passed through pipe l to a visbreaker coil 2 into a soaking drum I and through pipe 4 to fractionating towerl. An overhead distillate is removed from the fractionating tower'by means of outlet 0 and a side stream of gas oil from outlet I3.

The cracking is regulated so that the bottoms vconsist of a fuel oil having a gravity viscosity relationship such asv that of 8 A. P. I. gravity and a Furol viscosity of 1000 to 1400 seconds at 122 F. or of 9 A. P. I. and a Furol viscosity of 600 to 850 seconds at 122 F. Heavier or lighter bottoms having higher or lowerviscosities, respectively, may be used although the preferred range is'8 to 9? A. P. I. gravity. Within this range the quantity of material to be finally distilled is the minimum commensurate wlthease of handling a viscous solution. The fuel oil is removed through outlet 1, passed through heating coil 8, with or without the additionof steam through pipe 9 and flashed into a vacuum towerl I0, where an absolute presure of 25 to 100 mm. is maintained. Steam may be added to the coil I and to the bottom of the vacuum tower I0 by means of pipe il to aid in the distillation of the overhead distillate. It is preferred to add the major portion of the steam to the tower l0.

The

' used in the second heating coil 8 to heat the fuel oil is not above 800 F., preferably from 750 to 790 F. 'I'he conditions maintained are to avoid the formation of a carbon disulfide insoluble content in the bitumen.

Bitumen produced under these special conl ditions from Lagunillas crude of Venezuelan source is found to be most valuable in the preparation of plastics but minor portions of other similar type crudes may be added. The yields and equipment used may be varied, the latter may be batch as well as a continuous process.

Example 1 A Lagunillas and La Rosa mixture of crude.

having a gravity of 17.4 A. P. I. is cracked in the refinery in a so-called visbreaker without a soaker to obtain 58.4% of fuel-oil of a gravity of 8.9 A. P. I. and 11.4% of a pressure distillate of 400 F. end point naphtha. The fuel oil is vacuum reduced to obtain a bitumen of 402 softening-point and 1.266 specific gravity and 1.53% insoluble in carbon disulfide.

Example 2 A Lagunillas crude of about 17 A. P. I. gravity is subjected to a high temperature such as about 850 F. and a pressure not materially above 200 lbs. per sq. in., in a narrow confined stream in a coil and passed into a soaking drum. The cracked oil is then passed to a separator where an overhead distillate is recovered and bottoms of 8 A. P. I. gravity having a Furol viscosity of 1400 seconds at 122 F. is removed. This fuel oil is heated in a coil and passed to a separator using a flash zone pressure 86 mm. and steam to the extent of 19.25 pounds per barrel of feed stock added. The bottoms recovered is an asphalt havinga softening point of 370 F. and a susceptibility of 33.

Example 3 A mixture of a major part of Lagunillas crude and a minor part of La Rosa bottoms having a gravity of 17.1 A. P. I. were cracked in rening equipment under such conditions as tov give 14.4% of pressure distillate, 28.4% of gas oil and 57.2% of 9.1 A. P. I. gravityl bottoms. The 9.1 A. P. I. gravity bottoms were distilled under vacuum to a 402 F. softening point, 1.266 specific gravity, 1.53% insoluble in carbon disulde, susceptibility of 27 and satisfactory ductility.

The bitumens obtained by this process havel the desired susceptibility factor of 27 to 35 caiculated by the above formula. The advantage A further improved characteristic of this asphalt is that a higher softening point than that of gilsonite may be obtained. The proportion of bituminous material entering in the preparation of battery boxes is about 3.5%, the

other material being inert inorganic fillers, etc.

I claim:

1. A hard unoxidized bituminous. material adapted for use in a storage battery compound derived from cracked and vacuum .distilled paraftln-free asphaltic base petroleum crude oil having a susceptibilty factor between 27 and 35,

and a softening point between 320 F. and 420 F. and a content of material insoluble in carbon disulfide less than 1.5%.

2. A hard bituminous material adapted for V use in a storage battery compound derived from a cracked andv vacuum distilled West Venezuela f petroleum crude having a susceptibility 'factor between27 and 35 and a softening point between 320 F. and 420 F.

3. A hard bituminous material adapted for use in a storage battery compound derived from a cracked and vacuum distilled Lagunillas crude having a susceptibility factor between 27 and 35 and a softening point between 320 F. and 420 F.

4. Ahard bituminous material adapted for use as a storage battery compound derived from a cracked and vacuum distilled mixture ofLagunillas crude and La Rosa crude having a susceptibility factor between 27 and 35 and softening point between 320 F. and 420 F.

5. A hard bituminous Amaterial according to claim 4 in which the mixture from which the said bituminous material is prepared is invmaior part Iagunillas crude and in minor part La Rosa bottoms.

6. A process 'of preparing a hard bituminous material adapted for use in a' storage battery compound which comprises cracking a paraillnfree asphaltic base West Venezuela crude to a residual bottoms oil having a gravity viscosity relationship of 8 A. P. I. to 9 A. P. I. gravity vand Furol viscosity of between 1000 seconds and 1400 seconds to between 600 seconds and 850 seconds at 122 F. respectively, distilling the residual oil under vacuum to obtain a residue of bituminous material having a softening point in the range between 320 F. and 420 F. and susceptibility factor of 27 to 35.

7. A process of preparinga hardbituminous material adapted for use as a storage battery compound which comprises cracking a paraiiinfree asphaltic base Lagunillas crude to a residual bottoms oil having a gravity viscosity relationship of 8 A. P. I. to 9 A. P. I. gravityand Furol viscosity of between 1000 seconds and 1400 seconds to between 600 seconds and 850 seconds at 122 F. respectively, distilling the residual oil under vacuum to obtain a residue of bituminous material having a softening point in the range between 320 F. and 420 F. and susceptibility factor of 27 to 35.

8. A process of preparing a hard bituminous material adapted for use as a storage battery compound which comprises cracking a paraiiinfree asphaltic base mixture of a maior portion of yLagunillas crude and a vminor portion of La Rosa bottoms to aresidual bottom oil having a gravity viscosity relationship of 8 A. P. I. to 9 A. P. I. gravity and Furol viscosity of between 1000 seconds and 1400 seconds to between 600 seconds and 850 seconds at '122 F. respectively.'

distilling the residual oil under vacuum to obtain a residue ot bituminous material having a softening point in the range between 320 F. and 420 F. and susceptibility factor of 27 to 35.

9. A process of preparing a hard bituminous material adapted for use in storage battery compound Which comprises cracking a paraflin-free' asphaltic base Lagunillas crude to a residual bottom oil having a gravity viscosity relation` in the range between 320 F. and 420 F. and susceptibility factor of 27 to 35.

10. A process of preparing a hard bituminous material adapted for use in storage battery compound which comprises cracking a parafIln-free asphaltic base Lagunillas crude to a residual bottom oil having a gravity viscosity relationship of 8 A. P. I. gravity and Furol viscosity of between 1000 seconds and 1400 seconds at 122 F., distilling the residual oil under absolute pressure 25 to 100 mm. with 10 to 40 lbs. of steam per barrel of charge stock to obtain a residue of -bituminous material having a softening point in the range between 320 F. and 420 F. and susceptibility factor of 27 to 35.

11. A hard unoxidized bituminous material adapted for use in a storage battery compound derived from a mixture of cracked and vacuum distilled paraffin-free asphalticbase petroleum crude oils having a susceptibility factor between 27 and 35 and a softening point between 320 F. and 420 F. and a content of material insoluble in carbon disulde less than 1.5%.

HENRY M. NOEL. 

